CN105552375A - Carbon nanotube paste for lithium battery and preparation method for carbon nanotube paste - Google Patents
Carbon nanotube paste for lithium battery and preparation method for carbon nanotube paste Download PDFInfo
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- CN105552375A CN105552375A CN201510950204.6A CN201510950204A CN105552375A CN 105552375 A CN105552375 A CN 105552375A CN 201510950204 A CN201510950204 A CN 201510950204A CN 105552375 A CN105552375 A CN 105552375A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a carbon nanotube paste for a lithium battery and a preparation method for the carbon nanotube paste. The carbon nanotube paste comprises the ingredients of carbon nanotubes, carbon black, a surfactant, a thickening agent and a solvent, wherein the ratio of carbon nanotube: carbon black: surfactant: thickening agent: solvent is (3-10wt%): (0-8wt%): (0.1-1.3wt%): (0-1wt%): (80-96wt%); and the uniformly-dispersed uniform carbon nanotube paste is prepared based on the ratio through a mixing and stirring process. Under the effects of the surfactant and the thickening agent, a high-speed mechanical stirring mode and an ultrasonic stirring mode are combined, so that the dispersion degree of the conductive agent is greatly improved; and pre-fabrication for the paste is carried out for the carbon nanotube conductive agent that is difficult to disperse, so that a relatively good dispersion effect is achieved, the stirring requirement in the next step applied to the battery paste is lowered, and a relatively good mixing effect can be realized.
Description
Technical field
The invention belongs to technical field of lithium batteries, relate to a kind of lithium battery carbon nano tube paste and preparation method thereof.
Background technology
Because lithium ion battery has the advantages such as energy density is high, self discharge is little, cycle performance is superior, lithium ion battery is widely used in stand-by power supply, energy storage device, electric automobile, electric bicycle, electric tool.
Especially apply as electrokinetic cell, requiring higher to the combination property of battery, in order to improve the large current discharging capability of battery, reducing the internal resistance of battery, improve the cycle life of battery, in battery plus-negative plate material, add the conductive agents such as carbon black, carbon nano-fiber, carbon nano-tube.Wherein carbon nano-tube has good conductive capability, and in practical application, carbon nano-tube carries out electron transmission by being mutually built into network in basis material, and then realizes conduction.In this network, contact with each other between carbon nano-tube, or carbon nano-tube contacts with other materials with conductive characteristic, make carbon nano-tube effectively improve the large current discharging capability of battery.But the large molecule that carbon nano-tube is made up of carbon atom, is dissolved in any solvent hardly, is easy to assemble bunchy in the solution and reunites.Main manifestations is the high apparent activation energy that the winding that causes greatly of draw ratio and bigger serface cause.Insoluble and agglomeration traits hampers the application of its reality greatly, processes bad meeting and has the opposite effect in cell fabrication processes, therefore need effective preparation for processing to solve agglomeration traits.
Summary of the invention
The invention provides a kind of lithium battery carbon nano tube paste and preparation method thereof, solve the problem that carbon nano-tube is difficult to disperse in lithium battery applications, improve the dispersion effect of carbon nano-tube to greatest extent, improve the heavy-current discharge performance etc. of lithium battery further.
For achieving the above object, the technical solution used in the present invention is:
A kind of lithium battery carbon nano tube paste, carbon nano tube paste comprises following composition; Carbon nano-tube, carbon black, surfactant, thickener, solvent, its proportioning: carbon nano-tube: carbon black: surfactant: thickener: solvent=(3 ~ 10wt%); (0 ~ 8wt%); (0.1 ~ 1.3wt%); (0 ~ 1wt%); (80 ~ 96wt%), carbon nano tube paste adopts this component proportion to be prepared into homodisperse slurry according to mix and blend technique.
According to described lithium battery carbon nano tube paste, described carbon nanotube diameter is 5 ~ 160nm, and length is 5 ~ 25 μm, and specific area is 60 ~ 400m
2/ g; Black grain diameter is 20 ~ 70nm, and specific area is 25 ~ 260m
2/ g.
According to described lithium battery carbon nano tube paste, described surfactant is one or more in polyvinylpyrrolidone, polyethylene glycol, polyacrylic acid, acrylate copolymer; Thickener is sodium carboxymethylcellulose and/or hydroxyethylcellulose, and solvent is nitrogen methyl pyrrolidone and/or deionized water.
Prepare a method for described lithium battery carbon nano tube paste, mix and blend technique comprises dry powder premix, solution preparation, the stirring of slurry premix, hybrid mode circulation stirring, and concrete steps are as follows,
1. dry powder premix: after carbon nano-tube and carbon black are weighed in powder mixer premix, the time is 20 ~ 40 minutes;
2. solution preparation: add respectively in solvent after surfactant, thickener being weighed, adopts dispersion machine to be dispersed to dissolution homogeneity consistent, control temperature 20 ~ 50 DEG C in whipping process;
3. slurry premix stirs: add in agitator tank by the solution 10% ~ 30% prepared, then add the dry powder of premix and remaining solution simultaneously, stir while adding powder and solution, revolution mixing speed is 20 ~ 40 revs/min and high speed dispersion dish mixing speed 800 ~ 1600 revs/min, and mixing time is 60 ~ 90 minutes;
4. hybrid mode circulation stirring, size circulations flows through direction: high speed machine mixer → ultrasonic stirrer → high speed machine mixer, namely slurry flows into ultrasonic stirrer from the container of homogenizer, and then the container entering homogenizer is flowed out from ultrasonic stirrer, the speed of slurry flows ultrasonic stirrer is that 5 ~ 20L/min circulation continuous carries out with flow, the time of circulation stirring is 2 ~ 6 hours, and in whipping process, temperature controls is 20 ~ 50 DEG C.
According to the described method preparing lithium battery carbon nano tube paste, step 4. slurry stirs in high speed machine mixer high speed, and its revolution mixing speed is 20 ~ 40 revs/min and high speed dispersion dish mixing speed 1800 ~ 2600 revs/min; Slurry flows ultrasonic stirrer cavity carries out ultrasonic disperse, and ultrasonic frequency range is 15KHz ~ 50KHz.
Advantageous Effects of the present invention is; The pre-prepared of slurry is carried out to the carbon nanotube conducting agent being difficult to disperse, makes it reach good dispersion effect, reduce next step and be used in stirring requirement in cell size, good mixed effect can be reached; Wire and granular conductive agent combine, and have complementary advantages, can form good conductive network in battery pole piece, larger improves conductance ability; Under the effect of surface activity, thickener, adopt the mode that high speed machine stirs and ultrasonic agitation combines, conductive agent degree of scatter is improved greatly.
Accompanying drawing explanation
Fig. 1 anode pole piece SEM schemes.
Fig. 2 cathode pole piece SEM schemes.
Embodiment
Embodiment 1
For oiliness carbon nano tube paste and preparation method thereof, its formula and step as follows.
A kind of lithium battery carbon nano tube paste, the formula of employing is, carbon nano-tube: carbon black: polyvinylpyrrolidone: nitrogen methyl pyrrolidone=6wt%:3wt%:1.2wt%:89.8wt%.Wherein, carbon nanotube diameter is 7 ~ 15nm, and length is 6 ~ 15 μm, and specific area is 260m
2/ g.Black grain diameter is 30 ~ 50nm, and specific area is 60m
2/ g.
Mix and blend technique comprises dry powder premix, solution preparation, the stirring of slurry premix, hybrid mode circulation stirring, and concrete steps are as follows:
(1) dry powder premix: quality of carbon nano-tube and carbon black being weighed is respectively 6Kg and 3Kg, then doing time in advance in powder mixer is 40 minutes;
(2) solution preparation: quality of being weighed by surfactant polyvinylpyrrolidone is 1.2Kg, adds in solvent after weighing, solvent quality is 89.8Kg, adopts dispersion machine to be dispersed to dissolution homogeneity consistent, control temperature 20 ~ 50 DEG C in whipping process;
(3) slurry premix stirs: add in agitator tank by the solution prepared 10%, then adds the dry powder of premix and remaining solution simultaneously.While add powder and solution, limit is stirred, and revolution mixing speed is 30 revs/min and high speed dispersion dish mixing speed 1000 revs/min, and mixing time is 60 minutes;
(4) hybrid mode circulation stirring: size circulations flows through direction and is, high speed machine mixer → ultrasonic stirrer → high speed machine mixer, namely slurry flows into ultrasonic stirrer from the container of homogenizer, and then flows out the container entering homogenizer from ultrasonic stirrer.The speed of slurry flows ultrasonic stirrer is counted as 10L/min with flow, circulation continuous carries out, the time of circulation stirring is 6 hours, in whipping process, temperature controls is 20 ~ 50 DEG C, slurry stirs in mixer high speed, its revolution mixing speed is 40 revs/min and high speed dispersion dish mixing speed 2000 revs/min, and slurry flows ultrasonic stirrer cavity carries out ultrasonic disperse, and ultrasonic frequency range is 20KHz ~ 30KHz.
Slurry after preparation mixes with positive pole LiFePO 4 material, prepares lithium battery slurry and finally makes anode pole piece, and the SEM figure of pole piece as shown in Figure 1.Can find out that carbon nano-tube has good dispersion effect, carbon nano-tube and carbon black and positive electrode form good conductive network.
Embodiment 2
For water-based carbon nano tube paste and preparation method thereof, its formula and step as follows.
The formula adopted is, carbon nano-tube: carbon black: acrylate copolymer: sodium carboxymethylcellulose: deionized water=3wt%:1wt%:0.5wt%:0.2wt%:95.3wt%.Wherein, carbon nanotube diameter is 12 ~ 25nm, and length is 13 ~ 25 μm, and specific area is 160m
2/ g.Black grain diameter is 40 ~ 60nm, and specific area is 40m
2/ g.
Mix and blend technique comprises dry powder premix, solution preparation, the stirring of slurry premix, hybrid mode circulation stirring, and concrete steps are as follows:
(1) dry powder premix: quality of carbon nano-tube and carbon black being weighed is respectively 3Kg and 1Kg, then doing time in advance in powder mixer is 30 minutes;
(2) solution preparation: surfactant polyvinylpyrrolidone and thickener sodium carboxymethylcellulose are weighed, quality is respectively 0.5Kg, 0.2Kg, add after weighing in solvent, solvent quality is 95.3Kg, dispersion machine is adopted to be dispersed to dissolution homogeneity consistent, control temperature 20 ~ 50 DEG C in whipping process;
(3) slurry premix stirs: add in agitator tank by the solution prepared 20%, then add the dry powder of premix and remaining solution, while add powder and solution, limit is stirred simultaneously, revolution mixing speed is 20 revs/min and high speed dispersion dish mixing speed 800 revs/min, and mixing time is 90 minutes;
(4) hybrid mode circulation stirring: size circulations flows through direction and is, high speed machine mixer → ultrasonic stirrer → high speed machine mixer, namely slurry flows into ultrasonic stirrer from the container of homogenizer, and then flows out the container entering homogenizer from ultrasonic stirrer.The speed of slurry flows ultrasonic stirrer is counted as 5L/min with flow, circulation continuous carries out, the time of circulation stirring is 3 hours, in whipping process, temperature controls is 20 ~ 50 DEG C, slurry stirs in mixer high speed, its revolution mixing speed is 20 revs/min and high speed dispersion dish mixing speed 2400 revs/min, and slurry flows ultrasonic stirrer cavity carries out ultrasonic disperse, and ultrasonic frequency range is 25KHz ~ 35KHz.
Slurry after preparation and negative pole graphite material carry out being mixed with lithium battery slurry and finally make negative pole piece of battery, and as shown in Figure 2, can find out that carbon nano-tube has good dispersion effect, carbon nano-tube and graphite form good conductive network to the SEM figure of pole piece.
Embodiment recited above is only be described the preferred embodiment of the present invention; not design of the present invention and protection range are limited; under the prerequisite not departing from design concept of the present invention; the various modification that in this area, common engineers and technicians make technical scheme of the present invention and improvement, all should fall into protection scope of the present invention.
Claims (5)
1. a lithium battery carbon nano tube paste, is characterized in that: carbon nano tube paste comprises following composition; Carbon nano-tube, carbon black, surfactant, thickener, solvent, its proportioning: carbon nano-tube: carbon black: surfactant: thickener: solvent=(3 ~ 10wt%): (0 ~ 8wt%): (0.1 ~ 1.3wt%): (0 ~ 1wt%): (80 ~ 96wt%), carbon nano tube paste adopts this component proportion to be prepared into homodisperse slurry according to mix and blend technique.
2. lithium battery carbon nano tube paste according to claim 1, is characterized in that: described carbon nanotube diameter is 5 ~ 160nm, and length is 5 ~ 25 μm, and specific area is 60 ~ 400m
2/ g; Black grain diameter is 20 ~ 70nm, and specific area is 25 ~ 260m
2/ g.
3. lithium battery carbon nano tube paste according to claim 1, is characterized in that: described surfactant is one or more in polyvinylpyrrolidone, polyethylene glycol, polyacrylic acid, acrylate copolymer; Thickener is sodium carboxymethylcellulose and/or hydroxyethylcellulose, and solvent is nitrogen methyl pyrrolidone and/or deionized water.
4. prepare a method for lithium battery carbon nano tube paste described in any one of claim 1-3, it is characterized in that: mix and blend technique comprises dry powder premix, solution preparation, the stirring of slurry premix, hybrid mode circulation stirring, and concrete steps are as follows,
1. dry powder premix: after carbon nano-tube and carbon black are weighed in powder mixer premix, the time is 20 ~ 40 minutes;
2. solution preparation: add respectively in solvent after surfactant, thickener being weighed, adopts dispersion machine to be dispersed to dissolution homogeneity consistent, control temperature 20 ~ 50 DEG C in whipping process;
3. slurry premix stirs: add in agitator tank by the solution 10% ~ 30% prepared, then add the dry powder of premix and remaining solution simultaneously, stir while adding powder and solution, revolution mixing speed is 20 ~ 40 revs/min and high speed dispersion dish mixing speed 800 ~ 1600 revs/min, and mixing time is 60 ~ 90 minutes;
4. hybrid mode circulation stirring, size circulations flows through direction: high speed machine mixer → ultrasonic stirrer → high speed machine mixer, namely slurry flows into ultrasonic stirrer from the container of homogenizer, and then the container entering homogenizer is flowed out from ultrasonic stirrer, the speed of slurry flows ultrasonic stirrer is carried out with flow 5 ~ 20L/min circulation continuous, the time of circulation stirring is 2 ~ 6 hours, and in whipping process, temperature controls is 20 ~ 50 DEG C.
5. the method preparing lithium battery carbon nano tube paste according to claim 4, is characterized in that:
Step 4. slurry stirs in high speed machine mixer high speed, and its revolution mixing speed is 20 ~ 40 revs/min and high speed dispersion dish mixing speed 1800 ~ 2600 revs/min; Slurry flows ultrasonic stirrer cavity carries out ultrasonic disperse, and ultrasonic frequency range is 15KHz ~ 50KHz.
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Cited By (6)
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| CN108428865A (en) * | 2018-03-05 | 2018-08-21 | 天臣新能源研究南京有限公司 | A kind of preparation method of lithium ion battery anode slurry |
| CN109802088A (en) * | 2019-03-20 | 2019-05-24 | 江西理工大学 | One kind can fast charge lithium ion battery and preparation method thereof |
| CN109860538A (en) * | 2018-12-20 | 2019-06-07 | 天津市捷威动力工业有限公司 | A kind of lithium battery silicon-carbon cathode slurry and preparation method thereof, lithium ion battery |
| CN109921088A (en) * | 2019-03-20 | 2019-06-21 | 江西理工大学 | A kind of column lithium ion battery and preparation method thereof |
| CN111463490A (en) * | 2020-03-20 | 2020-07-28 | 梅州市量能新能源科技有限公司 | Preparation method of battery glue solution |
| CN112018328A (en) * | 2020-09-21 | 2020-12-01 | 珠海冠宇电池股份有限公司 | Silicon-doped negative plate and lithium ion battery comprising same |
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| CN112018328B (en) * | 2020-09-21 | 2021-07-06 | 珠海冠宇电池股份有限公司 | Silicon-doped negative plate and lithium ion battery comprising same |
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